Process of manufacturing anhydrids of fatty acids.



J. WEBER. v PROCESS OF'MANUFAOTURING ANHYDRIDS OF FATTY ACIDS.

APPLICATION FILED JUNE 30, 1911.

1.1 Patented Feb. 27, 1912 mltnasses; I Imam?- I WI Q i Y HMm-M his09650271265 UNITED ,STATES PATENT OFFICE} JOSE! WEBER, FESSEN-ON-THE-RUHR, GEBM IJAN Y.

PROCESS or menuracrunme Amnrpnms or mm? ACIDS.

'1'0 all whom it may concern:

Be it known that 1, Jose!" Vi-men, subject of the King of Prussia,(ierman Emperor, resident of Essen-on-the-Ruhr, in the German Empire,have invented a new and useful Process of Manufacturing Anhydrids ofFatty Acids, of which the following is an exact specification.

fatty acid salt or from a mixture of salts of This invention relates toan improved process of manufacturing'anhydrids of fatty acids,especially acetic anhydrld, from a out with much less trouble by mixinga fatty acid salt or salts in a dry state with sulfur, usually in theform of powder of sulfur or flowers of sulfur, and acting on thismixture with dry chlorin, good results having been obtained by takingthe materials in proportion, for example, of about 8 molecules ofacetate (ofa monobasic metal) to 1 atom of sulfur, these proportions,however, not being essential. In the process of the aforesaidapplication the reaction took place at a 7 lowtemperaturm-say at 20 (1.or less+ carrying out the process .of the aforesaid and. at that timethe carrying out ofthe .process at a'low temperature seemed to beessential. At the end of the operation of application-the productobtained by the reaction was moderately heated for some time in order totransform any fatty acid .chlorid stillpresent into anhydrid, afterwhich the anhydridwas eventually distilled in wmw in a manner'wellunderstood. I have found,

however, that in carrying out the process of the aforesaid application,especially with acetic anhydrid, tl e reaction on which said process isbased takes place not only at the low'temperatures above mentioned (asset forth in the prior application, but that,it also takes place, andthatit is possible to Specification of Letters Patent.

Application filed June 30, 1911. --Serial No. 688,137.

I Patented Feb. 27, 1912.

higher temperatures, if the mixture of the fatty acid salt or acetatewith sulfur is acted upon by chlorin in the presence of a suitablediluting or distributing substance, such for example as acetic anhydrid.The temperature upto which such reaction may take place with goodresults may be said to be An important advantage resulting from thecarrying out of thisimprovedprocess is that it is not necessary in thepresent case,- as it was in the process described in the aforesaidapplication, to maintain during the reaction temperatures which are onlyohtainable by the use of refrigerating machines. Thus in the presentcase, as these refrigerating machines are not required, both the processand the apparatus for carrying out the process are simplified in a highdegree, and by this simplification the manufacture of fatty acidanhydrid, and particularly acetic anhydrid, on a large scale isfacilitated and can be eli'ected at much lower cost than in the case ofthe process described in the former application.

In the drawing apparatus suitable for carrying out the improved processis illustrated.

Referring to said drawing, 2 designates a tightly closed reactionchamber or vessel into which the mixture to be acted upon has beenintroduced. A stirrer or means for keeping in motion the substanceforming the charge is illustrated at 3. It may be operated by anysuitable mechanism, such as that shown at 4-. The chlorin employed,which should be in a dry state, may be admitted at 5, and its flowregulated or varied 'as desired. as for example by means of a valve 6.The anhydrid resulting from the reaction will in this case leave thereaction vessel-through a pipe 7. which may also have 'a'valve 8therein, by means ofwvliichwommunication with the reaction vessel may bemade or cut off as required, The pipe 7 leads to the coils of acondenser 9, in which the anhydrid distilled over fromthe reactionvessel. 2 is condensed and from 'which the liquid distilled passes to areceiving-yessel 10. a t

g In order to make clear the manner in sel kilograms of carefully driedsodium which this process is practiced the following -1S given as oneexample: In the reactlonvesacetate are mixed with at least 16 kilogramsof sulfur or flowers of sulfur andan amount fatty aci of acetic anhydridequal to the uantity of sodium acetate used. The vesse [2 is thentightly closed and this mixture at a temperature of say 25 C., themixture being at the same time thoroughly stirred. If desired thereact-ion vessel may be exhausted before introducing the chlorin. Theintroduction of chlorin is so regulated that in say 5 hours at least106% kilograms V vessel. The chlorin admitted is quickly taken up by themixture and the pressure prevailin in the chamber 2 at the end of thereaction usually exceeds that at the beginning by only 'one tenth of anatmosphere or a little more. It is believed to be unnecessary toconsider whether in this reactionthe acetic anhydrid present only actsas a diluent or distributing means, or whether its action is a catalytlcone that results in advancing the reaction.

At the end of the reaction the resulting liquid anhydrid may bedistilled. substantially as in my aforesaid application. ,As in theformer case it is advlsable to hold a high vacuum during distillation,as it is only with the highest degree of vacuum that the output ofanhydrid will be' approximately the theoretical one, i. 204 kilograms.

What I claim is:

1. A process for the production of fatty acid anh drid, which consistsin mixing a d salt with sulfur, both being in a dry state, chlorin attem eratures up to 4050 C. in the'presence o a suitable diluent.

2. A rocess for the production of fatty acid'an ydrid, which consists inmixing a fatty acid salt with sulfur, both being in a dry state,

chlorin introduced into will have entered the reaction and; treating themixture with and treating the mixture with chlorin at temperatures up to4050 C. in

the presence of an anhydrid of a fatty acid.

3. A process for'the production of acetic anhydrid which consists inmixing an acetate with sulfur, both being in a dry state, and treatingthe mixture with chlorin at temperatures u to 40-50 C. in the presenceof, acetic anhy rid.

4. A process for the production of fatty acid anhydrid, which consistsin mixing a plurality of salts of the same fatty acid with sulfur, allbeing in a dry state, and treating the mixture with chlorin attemperatures up to 40-50 C, in the presence of a suitable diluent. g

5. A process for the production of fatty acid anhydrid, which consistsin mixing a plurality of salts of the same fatty acid with sulfur, allbeing in a dry state, and treating the mixture with chlorin attemperatures up to 40-50 C. in the'presence of an organic acid anhydrid.V 6. A process acid anhydrid, which consists in mixing a plum lity ofsalts of the same fatty acid with sulfur, all being in a dry state, andtreating the mixture with chlorin at temperatures-up to 4050 C. in thepresence of an anhydrid of the same fatty acid. y

7. A process for the production of acetic anhydrid, which consists inmixing a lurality of acetates with sulfur, all being in a dr state, andtreating the mixture with ch orin at temperatures up to 4050 C. in thepresence of acetic anhydrid.

, JOSEF WEBER. a 8.

Witnesses CHAS. J. WRIGHT, ALFRED HENKEL.

for the production .of fatty

